StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Hydrochloric Acid → 3,3-Bisfluoromethyl-1-(4-chlorophenoxy)-1-(imidazol-1-yl)-butan-2-ol

HRID 1649178
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1649178
[F:1][CH2:2][C:3]([CH2:21][F:22])([CH3:20])[C:4](=[O:19])[CH:5]([O:11][C:12]1[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][CH:13]=1)[N:6]1[CH:10]=[CH:9][N:8]=[CH:7]1.[BH4-].[Na+].Cl.C(=O)(O)[O-].[Na+]>CO>[F:1][CH2:2][C:3]([CH2:21][F:22])([CH3:20])[CH:4]([OH:19])[CH:5]([O:11][C:12]1[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][CH:13]=1)[N:6]1[CH:10]=[CH:9][N:8]=[CH:7]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 4311764Sodium borohydrideHCID 130194373,3-Bisfluoromethyl-1-(4-chlorophenoxy)-1-(imidazol-1-yl)-butan-2-one

Produkt 1

HCID 130194383,3-Bisfluoromethyl-1-(4-chlorophenoxy)-1-(imidazol-1-yl)-butan-2-olAusbeute 69,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

31.9 g (0.097 mol) of 3,3-bisfluoromethyl-1-(4-chlorophenoxy)-1-(imidazol-1-yl)-butan-2-one were dissolved in 600 ml of methanol, and 5.45 g (0.14 mol) of sodium borohydride were added in portions at 0° to 5° C. The mixture was subsequently stirred for 15 hours, 15 ml of concentrated hydrochloric acid were added and the mixture was stirred at room temperature for 2 hours. Thereafter, the reaction mixture was stirred into 800 ml of aqueous, saturated sodium bicarbonate solution. It was extracted with 1,000 ml of methylene chloride and the organic phase was washed twice with 1,000 ml of water each time, dried over sodium sulphate and concentrated by distilling off the solvent in vacuo. The oil which remained was stirred with isopropyl ether. 22.2 g (67.5% of theory) of 3,3-bisfluoromethyl-1-(4-chlorophenoxy)-1-(imidazol-1-yl)-butan-2-ol of melting point 137° C. were obtained. ##STR77##

Aufarbeitung

  1. stirringthe mixture was stirred at room temperature for 2 hours
  2. extractionIt was extracted with 1,000 ml of methylene chloride
  3. washthe organic phase was washed twice with 1,000 ml of water each time
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated
  6. distillationby distilling off the solvent in vacuo
  7. stirringThe oil which remained was stirred with isopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-991b89c3282a4cbbaacca3d3d2f14dee
Quelldatensatz
uspto-grants-1983_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04415586

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion